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Marshall Space Flight Center Research and Technology Report 2017

This report features over 60 technology development and scientific research efforts that collectively aim to enable new capabilities in spaceflight, expand the reach of human exploration, and reveal new knowledge about the universe in which we live. These efforts include a wide array of strategic developments: launch propulsion technologies that facilitate more reliable, routine, and cost effective access to space; in-space propulsion developments that provide new solutions to space transportation requirements; autonomous systems designed to increase our utilization of robotics to accomplish critical missions; life support technologies that target our ability to implement closed-loop environmental resource utilization; science instruments that enable terrestrial, solar, planetary and deep space observations and discovery; and manufacturing technologies that will change the way we fabricate everything from rocket engines to in situ generated fuel and consumables.

Research and Technology Report↗

Optimized Carbon Fiber Intermediate Development to Enable High-Volume Manufacturing of Lightweight Automotive Composites

The ongoing pursuit of improved fuel economy and reduced greenhouse gas emissions has resulted in sustained interest for lightweight materials technologies. In this context, carbon fiber composites have captured the imagination of automotive engineers due to the potential to achieve substantial mass reduction when compared to traditional steel construction. That stated, the use of carbon fiber composites in automotive has been limited for the most part to premium supercars and other derivative platforms. In these cases, manufacturing costs are less of an obstacle to implementation, and the performance benefits of carbon fiber have enabled production of structures offering more than 50% weight savings. In practice, translating these low-volume demonstrations onto high-volume vehicle platforms has remained challenging. This can be attributed to several factors, with the absence of suitable high throughput production methodologies being a key impediment. To date, structural, crash critical components have relied upon manufacturing techniques born out of the aerospace industry. This has created a disconnect between automotive production systems that are accustomed to manufacturing multiple parts per minute and the aerospace technologies that have cycle times in the order of hours. Consequently, the focus of this project is the development of manufacturing process technology for carbon fiber composites that can support a mainstream vehicle program at an assumed throughput of 100,000 vehicles per year. In practice, this translates to a part-to-part cycle time of less than 3 minutes. Project participation included contributions from a broad range of academic, industrial and national lab partners. The primary scope of work, being the development of new carbon fiber epoxy compounds that are stable at room temperature and suited to high throughput automated processing. For project management, the work streams were divided into six key areas, with the lead organization in parentheses. • Carbon fiber/epoxy materials formulation development and scale up (Dow) • Simulation of discontinuous near isotropic meso-structure intermediates (Purdue) • Simulation of mechanical performance of compression molded components (Purdue) • Meso-Scale morphological analysis and correlation with structural performance (UTK) • Paint and adhesion durability analysis (MSU) • Demonstrator part design, prototype production, and validation testing (Ford). The primary goal at the commencement of the project was development of a chopped carbon fiber sheet molding compound (SMC) that offered a three times improvement in tensile modulus over a comparable glass-based SMC. In addition to meeting mechanical performance targets, the resin kinetics were modified to achieve a processing cycle time of less than 3 minutes. Other critical-to-quality (CTQ) specifications were also stipulated to account for a broad range of materials and processing characteristics. To achieve the above, staff scientists at Dow Chemical created an extensive series of new epoxy blends for testing and validation. Throughout this development, a key challenge was attaining material performance goals without impacting processing behavior and paintability of finished components. The latter required a new internal mold release system being developed by Dow that was designed to complement the kinetics of the rapid cure epoxy. As a complement to work studies at the industrial partners, the teams from academia executed a series of analytical and experimental studies to investigate potential factors influencing CF-SMC performance. Unit cell models were developed to capture the meso-scale representations of the fiber matrix architecture. Results of this analysis and subsequent morphological investigations led to the design of a novel composite derivative comprising carbon fiber platelets embedded in an epoxy matrix; the platelet size and aspect ratio playing significant role in final composite properties. This approach was a departure from previous research in CF-SMC development whereby bulk filamentization or disassembly of the carbon fiber rovings had been considered the most effective means of achieving both fiber wet through and wet-out. As the course of the academia studies progressed, the aspect ratio of the fiber constituents was further optimized before finalizing material attributes and processing conditions. For the purposes of technology validation, the Ford team led a work stream devoted to the design, fabrication and testing of demonstration components. The carbon fiber SMC material has the potential to displace numerous stampings and castings on an automotive structure but ultimately vehicle closure applications were selected to showcase the abilities of the CF-SMC to achieve both mass reduction and business case for large complex structures. Using target properties established by the Dow staff scientists, the complete closure system for a full-size sedan decklid and a mid-size wagon liftgate were engineered. Prototypes for both applications were fabricated using production representative processing methods to allow for physical testing and performance validation of the CF-SMC structures. Following completion of a testing program that concluded with a FMVSS301 55 mph offset rear crash, the CF-SMC formulation was declared by the Ford team to have met all engineering requirements. To summarize, the joint development activities during this project led to significant technical breakthroughs and achievement of all milestones. The result was the development of a novel, tack-free carbon fiber molding compound that is suited to automated processing. This combined room temperature stability, fast cure kinetics, and internal mold release system facilitates cycle times that are conducive to high-volume production. The VORAFUSE M6400 successfully passed technology validation at Ford and is now eligible for consideration on future production commercial vehicle programs.

36 MATERIALS SCIENCE↗

Advancement of Novel Additively Manufactured Alloys for Space Applications

NASA has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. Several efforts have focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into development and flight applications. While many common aerospace alloys have been and continue to be a focus of ongoing development, the need for custom-alloy developments for high performance applications enabled by AM processes has been realized. The applications being targeted are liquid rocket engines with high heat fluxes, high pressure, and that utilize propellants such as hydrogen, which can degrade the alloy. NASA has recently focused on the development and advancement of novel alloy advancement using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, and JBK-75. These alloys have been evaluated using the laser powder bed fusion (L-PBF) and laser powder directed energy deposition (LP-DED) processes. The results from these processes have demonstrated that AM can enable rapid development of new alloy systems that can yield higher performances. These alloys have undergone the fundamental metallurgical evaluations, heat treatment study, and microstructure characterization and mechanical testing campaign. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL). This presentation will provide a background and overview of these AM-enabled novel alloys, AM processing development including metallurgical and mechanical property studies. It will also cover the latest advancement in the parallel component development and testing and future developments. The goal of these alloy development is to allow for technology infusion into NASA and commercial spaceflight missions as well as to establish and sustain the needed commercial AM supply chain.

Additive Manufacturing↗

Functional Photoresists for Energy Applications. Final Report

Monolithic ultralow-density porous bulk materials have recently attracted much interest due to many emerging applications in the areas of catalysis, energy storage and conversion, and thermal insulation. They are also important components of high energy density (HED) and inertial confinement fusion (ICF) targets. However, despite tremendous progress that has been made in the synthesis of porous materials, deterministic and independent control over microscopic architecture, density and composition remain key issues, and their integration in high precision devices requires cost and time-intensive mechanical machining that not only reduces reproducibility by generating debris but also limits the complexity of the 3D shapes that can be realized. In this project, we overcame these limitations by developing a universal templating capability that provides deterministic and independent control over density, composition, architecture, and macroscopic sample shape. This was achieved by developing the technology to 1) 3D print ultrahigh resolution, ultra-high precision polymeric micro-lattice templates, 2) coat these templates with the desired materials, and 3) removing the template (Fig. 1a). Atomic layer deposition (ALD) provides the atomic scale coating thickness accuracy required for precisely controlling density. While this templating approach had been demonstrated in prior work, limitations in suitable photoresists, 3D print technologies, print design, and template removal techniques did not allow the fabrication of millimeter-sized high-precision parts with sub-micron resolution. To enable this technology, we developed 1) two-photon polymerization (TPP) print designs that enable the fabrication of millimeter-sized, mechanically robust polymeric templates with sub-micron resolution and 2) a continuum level TPP printing simulation capability for additional print design guidance; 3) atomistic models to study photoresist polymerization kinetics and network topography, 4) refractive index matched polymeric and preceramic TPP photoresists, and 5) functional TPP photoresists including porous voxel structures and self-immolative polymer photoresist chemistries; and 6) damage free template removal techniques that enable the fabrication of defect-free high-precision low-density foam components. We also developed a templating approach for pure carbon microlattices with a unique tube-in-tube ligament morphology. As a test platform, we pursued the fabrication of foam liners that promise to further increase the neutron yield in indirect drive ICF experiments by improving implosion symmetry control and coupling between the laser and the deuterium-tritium fuel. This application requires fabrication and integration of a ultra-high precision, millimeter-sized, thin-walled (200-400 micrometer thick), low-density (10-30 mg/cc), high atomic number (high Z) cylindrical foam tube into the gold hohlraum of an indirect drive ICF target (Fig. 1b). While our hohlraum liner test case will mainly find application in HED and ICF experiments, the underlying science will also directly apply to previously developed nanoparticle and additive manufacturing technologies and will advance those techniques as well.

36 MATERIALS SCIENCE↗

Advancement of Metal Additive Manufacturing Processes and Alloys for Rocket Propulsion Applications

NASA has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the 2000’s. Several efforts have focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into development and flight applications. While many common aerospace alloys have been and continue to be a focus of ongoing development, the need for custom-alloy developments for high performance applications enabled by various AM processes has been realized. The applications being targeted are liquid rocket engines with high heat fluxes, high pressure, and that utilize propellants such as hydrogen, which can degrade the alloy. NASA has recently focused on the development and advancement of novel alloy advancement using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, and JBK-75. These alloys have been evaluated using powder bed fusion (PBF), directed energy deposition (DED), and solid-state AM processes. The results from these processes have demonstrated that AM can enable rapid development of new alloy systems that can yield higher performances across various metal AM processes. These alloys have undergone the fundamental metallurgical evaluations, heat treatment study, and microstructure characterization and mechanical testing campaign. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL). This presentation will provide a background and overview of various AM-enabled novel alloys, a comparison across the AM processes, and development including metallurgical and mechanical property studies. It will also cover the latest advancement in the parallel component development and testing and future developments. The goal of these alloy development and use of various AM processes is to allow for technology infusion into NASA and commercial spaceflight missions as well as to establish and sustain the needed commercial AM supply chain.

Additive Manufacturing↗

Metal Additive Manufacturing Developments for Propulsion Applications

NASA has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the 2000’s. Several efforts have focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into development and flight applications. While many common aerospace alloys have been and continue to be a focus of ongoing development, the need for custom-alloy developments for high performance applications enabled by various AM processes has been realized. The applications being targeted are liquid rocket engines with high heat fluxes, high pressure, and that utilize propellants such as hydrogen, which can degrade the alloy. NASA has recently focused on the development and advancement of novel alloy advancement using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, and JBK-75. These alloys have been evaluated using powder bed fusion (PBF), directed energy deposition (DED), and solid-state AM processes. The results from these processes have demonstrated that AM can enable rapid development of new alloy systems that can yield higher performances across various metal AM processes. These alloys have undergone the fundamental metallurgical evaluations, heat treatment study, and microstructure characterization and mechanical testing campaign. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL). This presentation will provide a background and overview of various AM-enabled novel alloys, a comparison across the AM processes, and development including metallurgical and mechanical property studies. It will also cover the latest advancement in the parallel component development and testing and future developments. The goal of these alloy development and use of various AM processes is to allow for technology infusion into NASA and commercial spaceflight missions as well as to establish and sustain the needed commercial AM supply chain.

Additive Manufacturing↗

High-throughput oxidation screening and down-selection of refractory high entropy alloys in the Al-Cr-Mo-Nb-Ta-Ti system

Rapid experimentation and characterization are ever-present needs in the discovery of high entropy alloys. High entropy alloy systems are difficult to survey with systematic composition sweeps using traditional synthesis methods. The number of distinct compositions in even a four-element system is experimentally intractable. Exploration of these, and higher-element systems, necessitates thermodynamic prediction coupled with an automated sample creation method and a rapid screening methodology to effectively down-select alloys with targeted properties. As a result, a high-throughput method for evaluating the oxidation performance of refractory high entropy alloys was developed and tested. The six-element system of aluminum, chromium, molybdenum, niobium, tantalum, and titanium was evaluated for single phase stability and short-duration oxidation resistance. Target compositions were initially determined via thermodynamic predictions of single-phase stability across a wide temperature range. A twenty-five-sample build plate was produced using directed energy deposition additive manufacturing. After fabrication, the twenty-five 1 cm 3 samples were heat treated and characterized for composition and phase identification. The build plate was exposed to a high temperature oxidizing environment at 1000 °C for three hours. After oxidation, the composition, morphology, and chemistry of the oxides formed were characterized. Of the twenty-five samples produced, nine exhibited a favorable oxidation response, from which a single-phase BCC alloy at a composition of Al 13 Cr 7 Mo 19 Nb 18 Ta 26 Ti 17 was identified as the alloy with the most protective oxidation coating with a thin, adherent oxide scale. Finally, the complete experimental down-selection—from machine setup to final alloy identification—required approximately 45 labor hours, demonstrating a rapid validation for alloy discovery.

Additive manufacturing↗

Mechanical Properties of Continuous Fiber Reinforced Zirconium Diboride Matrix Composites

Continuous fiber reinforced zirconium diboride matrix composites, SCS-9a-(RBSiCZrB2)matrix, are being developed for leading edge, rocket nozzle and turbine engine applications. Recently, the composite materials have been characterized for tensile properties to 1250 C, the highest temperature tested. The tensile properties are fiber dominated as the matrix is microcracked on fabrication, but favorable failure characteristic are observed. Compression and shear mechanical testing results will be reported if completed. The effects of fiber volume fraction and matrix density on mechanical properties will be discussed. The target applications of the materials will be discussed. Specific testing being performed towards qualification for these applications will be included.

Stuffle, Kevin↗

A Broadband Superconducting Detector Suitable for Use in Large Arrays

Cryogenic detectors are extremely sensitive and have a wide variety of applications (particularly in astronomy), but are difficult to integrate into large arrays like a modern CCD (charge-coupled device) camera. As current detectors of the cosmic microwave background (CMB) already have sensitivities comparable to the noise arising from the random arrival of CMB photons, the further gains in sensitivity needed to probe the very early Universe will have to arise from large arrays. A similar situation is encountered at other wavelengths. Single-pixel X-ray detectors now have a resolving power of (Delta)E < 5 eV for single 6-keV photons, and future X-ray astronomy missions anticipate the need for 1,000-pixel arrays. Here we report the demonstration of a superconducting detector that is easily fabricated and can readily be incorporated into such an array. Its sensitivity is already within an order of magnitude of that needed for CMB observations, and its energy resolution is similarly close to the targets required for future X-ray astronomy missions.

Day, Peter K.↗

Compact Micromachined Infrared Bandpass Filters for Planetary Spectroscopy

The future needs of space based observational planetary and astronomy missions include low mass and small volume radiometric instruments that can operate in high radiation and low temperature environments. Here we focus on a central spectroscopic component, the bandpass filter. We model the bandpass response of the filters to target the wavelength of the resonance peaks at 20, 40, and 60 micrometers and report good agreement between the modeled and measured response. We present a technique of using common micromachining processes for semiconductor fabrication to make compact, free standing resonant metal mesh filter arrays with silicon support frames. The process can accommodate multiple detector array architectures and the silicon frame provides lightweight mechanical support with low form factor. We also present a conceptual hybridization of the filters with a detector array.

Merrell, Willie C., II↗

Development of Inspection for Friction Stir Welds for Rocket Fuel Tanks

During development of the Ares I weld processes nondestructive and destructive testing were used to identify and characterize defects that occurred. These defects were named and character noted. This catalogue of defects and characteristics was then used to develop inspection methods for Self Reacting Friction Stir Welds (SR ]FSW) and Conventional Friction Stir Welds (C ]FSW). Dye penetrant, eddy current, x ]radiography, single element ultrasonic, and phased array ultrasonic (PAUT) inspection procedures were developed to target the expected defects. Once the method procedure was developed a comparison was performed to allow for selection of the best inspection method. Tests of the effectiveness of the inspection were performed on purposely fabricated flawed specimens and electrodischarge machined notches. The initial test results prompted a revisit of the PAUT procedure and a redesign of the inspection. Subsequent testing showed that a multi ]angle PAUT inspection resulted in better detection capability. A discussion of the most effective orientations of the PAUT transducer will be presented. Also, the implementation of the inspection on production hardware will be presented. In some cases the weld tool is used as the transducer manipulator and in some cases a portable scanner is used

Russell, Samuel S.↗

Electrical, thermal, and mechanical properties of spatially tailored fiber orientations in 3D printed carbon-carbon composites for EFAS/SPS

Using C-C synthesized at INL from continuous fiber 3D printed preforms, tooling was fabricated, tested, and compared to graphite. The anisotropic properties of the C-C material were leveraged to make stronger and more energy efficient tooling. Future work involves tailoring the fiber orientations to create targeted heating zones and thermal gradients.

36 MATERIALS SCIENCE↗

One–Step Fabrication of Nanocrystalline Nanonetwork SnO 2 Gas Sensors by Integrated Multilaser Processing

An integrated multilaser process is developed to fabricate nanocrystalline nanonetwork SnO 2 gas sensors in one integrated procedure, which combines electrodes fabrication, nanomaterials deposition, and postannealing. Interdigit electrodes are fabricated on an Au-coated fused silica substrate using a picosecond (ps) laser, which ablates the Au coating from the back of the substrate to pattern the electrodes. A novel transmitted Ps laser deposition (TPLD) process is designed to deposit SnO 2 nanonetwork on the interdigit electrodes with precise deposition area control under a close target-to-substrate distance. The obtained SnO 2 nanonetwork is in situ postannealed by a CO 2 laser to improve the crystallinity, while the nano morphology and grain size keep intact. To investigate the morphology and formation process of the nanonetwork, the microstructure of the laser-deposited SnO 2 layer is characterized. As a result, the crystallization control of CO 2 laser annealing is investigated through analyzing the Raman spectrum, X-ray diffraction (XRD) patterns, and lattice structures of the samples. By exposed to H 2 atmosphere, the fabricated gas sensor is demonstrated for H 2 monitoring.

08 HYDROGEN↗

Processing and Properties of a Phenolic Composite System

Phenolic resin systems generate water as a reaction by-product via condensation reactions during curing at elevated temperatures. In the fabrication of fiber reinforced phenolic resin matrix composites, volatile management is crucial in producing void-free quality laminates. A commercial vacuum-bag moldable phenolic prepreg system was selected for this study. The traditional single-vacuum-bag (SVB) process was unable to manage the volatiles effectively, resulting in inferior voidy laminates. However, a double vacuum bag (DVB) process was shown to afford superior volatile management and consistently yielded void-free quality parts. The DVB process cure cycle (temperature /pressure profiles) for the selected composite system was designed, with the vacuum pressure application point carefully selected, to avoid excessive resin squeeze-outs and achieve the net shape and target resin content in the final consolidated laminate parts. Laminate consolidation quality was characterized by optical photomicrography for the cross sections and measurements of mechanical properties. A 40% increase in short beam shear strength, 30% greater flexural strength, 10% higher tensile and 18% higher compression strengths were obtained in composite laminates fabricated by the DVB process.

Hou, Tan-Hung↗

Bench-Scale Testing of Monolithic PPI Structured Contactors for Direct Air Capture of CO 2

The overall project objective was to develop, optimize and bench-scale test the integrated embodiment of a leading direct air capture (DAC) sorbent composition, linear-poly(propylenimine) (l-PPI), in a structured material system, specifically a monolithic contactor for achieving low pressure drop, to justify its further scale-up in a subsequent program. The project team was led by CORMETECH, a leading monolithic gas/solid contactor manufacturer for environmental applications, and included Global Thermostat, a well-known DAC start-up, and Georgia Tech, a prominent US academic institution in carbon capture and DAC. The monolithic contactor for l-PPI in this project employed an advanced, cost-effective fabrication technique from CORMETECH, namely a porous monolith substrate directly impregnated with the amine, an approach contrasting to the traditional wash-coating methods used for activating monoliths. The l-PPI monolithic contractor is targeted for use in DAC systems such as the Global Thermostat DAC process, which involves the cyclic operation of ambient air flow over a monolithic amine contactor followed by steam-mediated thermal desorption and CO 2 collection, maximizing volumetric productivity while reducing the auxiliary power required to capture CO 2 from air. The Global Thermostat DAC process currently utilizes poly(ethyleneimine) (PEI) materials as baseline sorbents, which are subject to oxidative degradation and slow capacity fade at the elevated temperature required for efficient CO 2 removal. Georgia Tech, with Global Thermostat, had discovered in lab-scale efforts that l-PPI had superior resistance to oxidative degradation compared to PEI, with similar CO 2 adsorption capacity. While the novel l-PPI sorbent offers significant advantages over PEI for DAC, including potential design simplification and increased process efficiency, it is not commercially available, and prior to this project, had not yet been evaluated on the bench-scale in a structured contactor.

36 MATERIALS SCIENCE↗

Flat-plate module efficiency versus cost tradeoffs

The Five Year Research Plan energy cost methodology and in depth analyses based on the extensive data that are relevant to PV systems are used to facilitate the accomplishment of the $0.15/kWh energy cost goal. An equation is given for the five year energy cost methodology. The allocation guidelines are designed to be consistent with flat solar array (FSA) milestones for module cost, module efficiency, and the programmatic goal for energy cost. They are research targets that appear to be achievable, given prior accomplishments and planned activities in the areas of low cost silicon purification, low cost sheet material, high efficiency cell processing, low cost, long life encapsulants, and automated fabrication method. Extensive sensitivity analysis work has been performed that shows that these guidelines represent an efficient way to meet the intent of the DOE program.

Aster, R. W.↗

Ultra-stable, low phase noise dielectric resonator stabilized oscillators for military and commercial systems

EPSD has designed, fabricated and tested, ultra-stable, low phase noise microwave dielectric resonator oscillators (DRO's) at S, X, Ku, and K-bands, for potential application to high dynamic range and low radar cross section target detection radar systems. The phase noise and the temperature stability surpass commercially available DROs. Low phase noise signals are critical for CW Doppler radars, at both very close-in and large offset frequencies from the carrier. The oscillators were built without any temperature compensation techniques and exhibited a temperature stability of 25 parts per million (ppm) over an extended temperature range. The oscillators are lightweight, small and low cost compared to BAW & SAW oscillators, and can impact commercial systems such as telecommunications, built-in-test equipment, cellular phone and satellite communications systems. The key to obtaining this performance was a high Q factor resonant structure (RS) and careful circuit design techniques. The high Q RS consists of a dielectric resonator (DR) supported by a low loss spacer inside a metal cavity. The S and the X-band resonant structures demonstrated loaded Q values of 20,300 and 12,700, respectively.

Mizan, Muhammad↗

Nanoscale Test Strips for Multiplexed Blood Analysis

A critical component of the DNA Medicine Institute's Reusable Handheld Electrolyte and Lab Technology for Humans (rHEALTH) sensor are nanoscale test strips, or nanostrips, that enable multiplexed blood analysis. Nanostrips are conceptually similar to the standard urinalysis test strip, but the strips are shrunk down a billionfold to the microscale. Each nanostrip can have several sensor pads that fluoresce in response to different targets in a sample. The strips carry identification tags that permit differentiation of a specific panel from hundreds of other nanostrip panels during a single measurement session. In Phase I of the project, the company fabricated, tested, and demonstrated functional parathyroid hormone and vitamin D nanostrips for bone metabolism, and thrombin aptamer and immunoglobulin G antibody nanostrips. In Phase II, numerous nanostrips were developed to address key space flight-based medical needs: assessment of bone metabolism, immune response, cardiac status, liver metabolism, and lipid profiles. This unique approach holds genuine promise for space-based portable biodiagnostics and for point-of-care (POC) health monitoring and diagnostics here on Earth.

Chan, Eugene↗